Trospium chloride synthesis process
A technology of trospium chloride and synthesis process, which is applied in the field of pharmaceuticals to achieve the effects of short reaction steps, strong atom economy and low production cost
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Embodiment 1
[0028] Embodiment 1: the concrete steps of a kind of trospium chloride synthetic technique of the present invention are as follows:
[0029] 1. Preparation of diphenylglycol chloride: 50 g of diphenylglycolic acid and 130 g of thionyl chloride were added to the reaction flask, refluxed for 5 hours, and the unreacted thionyl chloride was reclaimed under reduced pressure, then recrystallized by adding n-hexane to obtain Diphenylglycol chloride 49g, yield 93%;
[0030] ② Preparation of nortropine alcohol: In an autoclave, add 100 g of α-tropine alcohol, dissolve in 500 mL of methanol, add 1 g of 10% Pd / C, 50 g of hydrochloric acid, replace with nitrogen, then pass hydrogen to 1 atm, and heat up to 60 ℃, heat preservation reaction for 2 hours, lowered to room temperature, filtered out the catalyst after pressure relief, and evaporated the solvent under reduced pressure to obtain 33 g of nortropine alcohol, with a yield of 73%;
[0031] ③Preparation of (3α-nortropine alcohol)-8-sp...
Embodiment 2
[0033] Embodiment 2: the concrete steps of a kind of trospium chloride synthetic technique of the present invention are as follows:
[0034] ①Preparation of diphenylglycol chloride: Add 50g of diphenylglycolic acid and 150g mL of thionyl chloride into the reaction flask, reflux for 5 hours, recover unreacted thionyl chloride under reduced pressure, then add n-hexane for recrystallization, Obtain 50 g of diphenylglycol chloride, yield 93%;
[0035] ② Preparation of nortropine alcohol: In an autoclave, add 100 g of α-tropine alcohol, dissolve in 500 mL of methanol, add 1.5 g of 10% Pd / C, 50 g of hydrochloric acid, replace with nitrogen, then pass hydrogen to 1 atm, and heat up to 60°C, heat preservation reaction for 2 hours, lower to room temperature, filter out the catalyst after pressure relief, and evaporate the solvent to dryness under reduced pressure to obtain 30 g of nortropine alcohol, with a yield of about 66%;
[0036] ③ Preparation of (3α-nortropine alcohol)-8-spiro-...
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